Document jyvrNGRN9NaRvjJ1njDaNDZQp
PROTOCOL
DETERMINATION OF THEOMFELPTRIONSG POINT/MELTING : RANGE
(OECD Guidelinefor TesoftChi emin calgs, 103
`Melting Poin/Melting Range
3M Lab Request No. U2723
`Submitted to
3M Corporation
`Environmental Laboratory
P.O. Box 33331 `St. Paul, Minnesota 55133
WILDLIFE INTERNATIONAL LTD.
8598 Commerce Drive
Easton, Maryland 21601
(410) 822-8600
December 2, 1998 PROTOCOL NO.: 454/120298/103/SUB454
3MLAB.REQUEST?
WILDLIFE INTERNATIONAL LTD.
-2-
DETERMINATION OF THE MELTING POINT/MELTING RANGE OF PFOS
`SPONSOR:
3M Corporation Environmental Laboratory
P.O. Box 33331 `St. Paul, Minnesota 55133
SPONSOR'SREPRESENTATIVE: TESTINGFACILITY:
Ms. Susan A. Beach.
`Wildlife International Ltd.
8Ea5s9t8oCnoMmamreyricanedDr2i1v6e01
STUDYDIRECTOR:
Ronda Jacobs `Senior Chemist
LABORATORYMANAGEMENT:~~ Willard B. Nixon, Ph.D.
`Manager of Chemistry
I
FORLABORATORYUSEONLY
Proposed Dates:
E| xSpereimeental --L8OTP20 ExTpeeormiimmeinotnalDue: 8 DecDec 92 |
| peieave: _4SUC 10C___ tamu pe times |
| testSubstantcoe: LFS Rocsiptoue"_299.0ct
PROTOCOLAPPROVAL
7
Y DIRECTOR
Millie
RATORY
(AGEMENT
Loa(od `SPONSOR'S REPRESENTATIVE
PROTOCOLNO.: 454/120298/103/SUB454
8 Lo 92
DATE
V/s
DATE
a )2[9R
DAT
3M LAB 000047 REQUEST NO. U2723
WILDLIFE INTERNATIONAL LTD.
3.
INTRODUCTION Wildlife International Ltd. will determine the melting point or melting range of PFOS (perfusulofornicoaciod,pcotatssaiumnsael).Thestudywillbeconducted attheWildlife International Lidanalytical chemistryfacilityinEaston,Maryland.Thestdywillbeperformedfollowingprocedures inOECDGuideline forTestingofChemicals, 102,Melting PoinMeltRianngge (1). Rawdataforall workperformedatWildlifeIntemationalLtd.and acopyofthefinalreportwillbefiledbyproject `numberinarchiveslocatedatWildlifeInternationalLid.orat analternativelocationtobespecifiedin thefinal report.
PURPOSE
"Thepurpossofthisstudyi todeterminethemeltingpointormeltingrangeof PFOS.
EXPERIMENTALDESIGN Themeltingpoist idefinedasthetemperatureatwhich thephasetransitionfrom asolidto a liquidsateat atmosprpeshsureeorcciurcs. Forsomesubstances,thetransitionoccursover arangeof tempdeefinre aastthemueltringeransge.Subsamplesofthetestsubstance illbe heatedin amelting pointtubeina temperature<ontrolledbeatingblockcontaining ameltingpointcapillry. Measurement ofmeltingpoints willbelimitteod 400C (approximately 673K), themaximumspecified for the: instrumentationused. Thetemperatureatwhich fiedropletsadbere uniformlytothewllofthemelting `pointtubewillbo accepteda themeltingpoint.Ifarangeoftemperatureisnotedbetweentheformation ofthefinedroplets(beginning ofmelting)an transition0:liquid (endofmelting), ameltingrangewill bereported.
MATEARNDIMAETLHODSS
TestSubstance
"The Sponsorwillbeaskedtoprovidethefollowinginformationconcerningthetestsubstance,
ifavailable:
L`otoCr BhatNceahmNemu(mobiredrescignaatilon) ~~EmCpoimrpiosciatlifoonr(mfuolrmausl)ti-componentmixtures)
Purity
Expiration Date
Theatached form IDENTIFICATION OFTEST SUBSTANCE BY SPONSOR (Appendix I) itobeused 0provideavailabeinformation. The Sponsoris responsibleforinformationon thepurity andcompositionofthetestsubstance,aswellasalinformation relatedtothesafehandlingofthetest
PROTOCOLNO.: 454/120298/103/SUB4S4
3MLABREQUEST NO, U2723
000048
WILDLIFE INTERNATIONAL LTD.
_a-
substance. The Sponsoralsoagreestoacceptanyunusedtestsubstanceo tetsubstancecontainers remaat thieenndofithenstugdy.
TestProcedure: "Themelingpointorrangevillbedeterminedusinga BuchiMeling PointB-540instrumentwith
meltingpointtubessuppliedbyBichi.Theinstrumentwillbecalibratedpriortousewith aminimum oftworeferencestandards.Subsamplesofthetestsubstancewillbetransferredto aminimumofthree.
capillarytubesto adepth ofapproximat3emlmy.Tubes willbetampedto packthetestsubstance.
Followinganinitialrapidscan(s) todetermine anapproximatemeltingpoint,theinstrumentvillbe programmedtoincrementthetemperatureoverthemeltingpointorrangeat a atenottoexceed 1Clmimite, Thetemperatureatwhichfiedropletsuniformlyadheretothetubewallwillbeaccepted a5themeltingpoint.I thetemperatureincreasessignificantly(spproximat2elCyormore)between theformationofthe inedropletsadheringtothetubewallsuntilliquification,ameltingrangewillbe
reported.
`Themeltingpointorrangewillberecord in Candreportedbothin Cand K.Thebarometric pressurevil berecordedatthetimeofmeasurementofthemeltingpointo range.
`SampleHandling andSafety: "TheSponsorwillidentifyanyspecial handlingorsafetyprecautions obeusedwiththeabove.
refetresetsnubsctaencde. Allnormalprecautionswithrespecttohandlingandstoragewillbetake.
`SamploandTestSubstance Retention Uponcompletionoftesting,portionsofthetestsubstanceusedaspartofthisstudywillbe
disposedofin accordance withfederal, tateandlocalregulations.Anyunusedportion ofthetest substancewillbereturnedtothe Spousor.
RECTO BOEMR AIND TAIS NED Rocordstobemaintained fordatageneratedbyWildifeInternationalLud.willinclude,butnot belimitetod: 1. Acopyofth signedprotocol. 2. Identificationandcharacterization ofthetestsubstance, if providedbytheSponsor. 3. Datesofinitiationandcompletion ofthestudy.
PROTOCOL NO: 454/120298/103/SUB454
3MLABREQUESTNO. U2723
000049
WILDLIFE INTERNATIONAL LTD
-5-
4. Datesofexperstiartmanedtn ermtinaatioln.
5. Storageconditionsofth test substance.
:
6. Testsubstanceulsoeg
7. Theinstrumenttemperatureprogram.
8 Individualandmeanmelingpoint measurcementsexpressedin Cand K.
9. Statisticalcalculations.
10. Testconditions.
11. Acopyofthefinalreport.
FINALREPORT
AfinalreportoftheresultsofthestudywillbepreparedbyWildlifeIntemationalLtd.Thereport
`willinclude,butnotbelimitedtothefollowing,when applicable:
1. Nameandaddressofthefacilityperformingthestudy.
2.
3.
Datesuponwhichthestudywasinitiated andcompleted.
A statementofcompliance signed by the Study Director
addressing
any
exceptions
to
Good.
LaboratoryPractice Standards
4. Purposeandprocedure,asstated intheapprovedprotocol,includingallamendmentsand
devitaottheiprootoncosl.
5. Thetestsubstanceidentification,includingname,chemicalabstractnumberorcodenumber,
`purity, composition, empirical formula, molecular formula, manufacturer's lot/batch number,
dissociationinwater,method ofanalysis,orotherinformationprovidedbythe Sponsor.
6. Descriptionofthetestmethodorreferencetothe methodusedalongwithanymodificationsmade.
7. Individual andmeanvalues obtainedforthemelting pointorrangeexpressedin Cand K.
8. Descriptionofany problemsexperiencedandhowtheywereresolved. 9. Astatementpreparedbythe QualityAssurance Unit listingthedatesthatstudy inspectionsand
`audits were madeand any findings thatwere recorded.
CHANOFGPRIOTNOCGOL
`Plannedchangestotheprotocolwillbeintheformof writtenamendmentssignedbythe Study
Dirae ndtchet Spoonsorr. Amendmentswillbeconsideredaspartoftheprotocolandwillbeattached
tofintal prhotoceol. Aayotherchanges willbein theformofwrittendeviations filedwiththeraw data. Allchangestotheprotocolwillbeindicatedinthefinalreport.
PROTOCOLNO.: 454/120298/103/SUB454
3MLABREQUENSOT. U2723
000050
WILDLIFE INTERNATIONAL LTD.
-6GOODLABORATORY PRACTICES
"This studywillbeconductedaccordingtotheGoodLaboratoryPracticesdescribedin OECD
(ISBN 92-84-12367-9)andEPA (40 CFR Parts 160 and/or 792). Eachstudyconductedby Wildlife InternatioLnuadl. i routinely examinedbytheWildifeIntemationalLtd.QualityAssuranceUnitfor compliancewith GoodLaboratoryPractices, StandardOperatingProceduresandthespecifiedprotocol AstatementofcompliancewithGoodLaboratoryPracticeswillbepreparedforallportionsof thestudy conbydWilduiifec Intet matieonalLdtd.The SponsorwillberesponsibleforcompliancewithGood
`LaboratoryPracticesfocproceduresperformedby otherlaboratories.Rawdataforallworkperformed
atWildlifeInternationalLtd.and acopyof the inalreport willbefledbyprojectnumberin archives TocatedontheWildlife IntemationalLid.siteoratanaltemativelocationtobespecifiedinthefinal report.
PROTOCOL NO: 454/120298/103/SUB4S4
3M LABREQUEST NO. U2723
000051
WILDLIFE INTERNATIONAL LTD. 7.
REFERENCES
1. OrCganhisateioMnmelftoiringEPcocoinnotamMieclliCnogospRearna,gtieo.nandDevelopment. 102. GuidfoerTlesitinngoef
PROTOCOLNO.: 454/120298/103/5UB454
3MLABREQUEST NO. U2723
000052
WILDLIFE INTERNATIONAL LTD.
-8-
APPENDIX I IDENTIFICATION OFTEST SUBSTANCE BY SPONSOR
To be Completed by Sponsor
I Test Substance Identity (nametobeusedinthereport): Fiffygroostane Sulfon Acid.Potassium Salt
Sample Code or Batch Number:Lat217 Pur(%iActtiyve Ingredient): 98.9%.
`Expiration Date: _2008
nbd somgh ry mn IL Test Substance Characterization
`Hthaeiv dente ity, streng urity andcompooros thei r cht aracitero istn ics
tothe startof this studyin accowirth d GLPaStn andcardes?
Yes___ No X_
IL Test Substance Storage Conditions
Pleaseindicatetherecommendedstorageconditionsat WildlifeInternational Ltd.
Ambintrobmtempenuee,
`Hasthestability ofthetestsubstance underthesestorageconditions
`been determinedinaccordancewith GLP Standards?
Yes __ No_ X_
Otherpertinent stability information:
IV. Toxicity Information:
Mammalian: RatLDSO 251mekgMouseLDSONA.
Aquatic:
Invertebrate Toxicity (EC/LCS0)
FishToxicity (LCS0)
s0 emsps 0 `OtherToxicity Information(includingfindingsof chronicandsubchronictests):
PROTOCNOOL 454/120098/10R3/aSs1a
war am ome bE
BOILING POINT
TEST SUBSTANCE
Identity: PFeCr-f9l5u.oro(o1c-tOacnteasnuelsfuolnfaotnei;c macaiyd,a1l,s1o,2b.e2.r3e,f3e.r4r,e4d,5t,o5,a6s.6P.F7.O7.S8.o8r.8heptadecaflucro-, potassium salt, CAS # 2795-39-3)
Remarks:
Testing was not conducted. Boiling point would be in excess of 400C.
000054